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US20180061540A1 - Method for producing a sintered r-iron-boron magnet - Google Patents

Method for producing a sintered r-iron-boron magnet Download PDF

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Publication number
US20180061540A1
US20180061540A1 US15/690,238 US201715690238A US2018061540A1 US 20180061540 A1 US20180061540 A1 US 20180061540A1 US 201715690238 A US201715690238 A US 201715690238A US 2018061540 A1 US2018061540 A1 US 2018061540A1
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Prior art keywords
magnet
powder
rxe
treated
sintered
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Inventor
Qingkai Wang
Dongdong Li
Guoqiang GENG
Mingjie Zhang
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Yantai Zhenghai Magnetic Material Co Ltd
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Yantai Zhenghai Magnetic Material Co Ltd
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Assigned to YANTAI ZHENGHAI MAGNETIC MATERIAL CO., LTD. reassignment YANTAI ZHENGHAI MAGNETIC MATERIAL CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GENG, GUOQIANG, LI, DONGDONG, WANG, QINGKAI, ZHANG, MINGJIE
Publication of US20180061540A1 publication Critical patent/US20180061540A1/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/026Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/0536Alloys characterised by their composition containing rare earth metals sintered
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/06Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
    • H01F1/08Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
    • H01F1/086Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together sintered
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0206Manufacturing of magnetic cores by mechanical means
    • H01F41/0246Manufacturing of magnetic circuits by moulding or by pressing powder
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0293Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • B22F2007/042Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
    • B22F2007/047Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method non-pressurised baking of the paste or slurry containing metal powder

Definitions

  • the invention relates to a method for producing a sintered R-Iron-Boron (R—Fe—B) magnet.
  • Grain boundary diffusion methods including evaporation process and contact process, are widely used to improve the coercive force of sintered Nd—Fe—B magnets.
  • the temperature of the evaporation process is difficult to control. If the temperature is too low, it is difficult for the heavy rare earth vapor to diffuse into the interior of magnets, leading to long treatment time. If the temperature is too high, the speed of producing heavy rare earth vapor is faster than the speed of vapor diffusing into the interior of magnets, leading to a poor grain boundary diffusion effect.
  • a heavy rare earth film is coated on the surface of magnets, destroying the surface condition of the magnets.
  • the surface coating requires to be removed, which involves complex operations and increases the costs.
  • a method for producing a sintered R—Fe—B magnet comprising:
  • the heavy rare earth element powder RX, the organic solid EP and the organic solvent ET are used to prepare the slurry RXE; the evenly-stirred slurry RXE is coated on the surface of the treated magnet; after a drying treatment, an RXE layer is formed on the surface of the magnet to realize the effect of arranging heavy rare earth elements on the surface of the magnet.
  • the RXE layer can be arranged on the surface of the magnet through brush coating, dipping, roller coating and spray painting.
  • the RXE layer is highly controllable in thickness and uniformity, is not easy to fall off and is easy to realize batch production. Since the heavy rare earth element RX is wrapped by the organic solid powder EP after drying treatment, the RXE layer on the surface of the magnet is not easy to oxidize. Therefore, the magnet can keep stable in the air for a long time.
  • the organic solid powder EP and the organic solvent ET are separated from the magnet so the content of carbon in the magnet will not increase significantly.
  • step (3) the slurry RXE needs to be stirred in use. Since the density of the powder RX is much greater than that of EP and ET, the slurry RXE still cannot keep stable and uniform for a long time although the organic solid EP used in the thick liquid prevents the powder RX from settling obviously. Therefore, the slurry RXE is stirred preferably in use.
  • the weight percent of the RX in the slurry RXE ranges from 30 wt. % to 90 wt. %.
  • the weight percent of the RX in the slurry RXE is too low, since the density of the powder RX is higher, the distribution uniformity of the RX in the slurry RXE lowers even if stir treatment is carried out so that the RX on the surface of the treated magnet is not even in distribution.
  • the weight percent of the RX in the slurry RXE is too high, the flowability of the thick liquid becomes lower and the viscosity of the thick liquid becomes higher so it is not easy to arrange an RXE layer which is even in thickness on the surface of the treated magnet.
  • step (3) the slurry RXE is arranged on the surface of a regular square magnet through brush coating and roller coating.
  • the slurry RXE is arranged on the surface of an irregular magnet through dipping and spray coating.
  • the slurry RXE forms an RXE layer which is even in thickness on the surface of the magnet through brush coating, roller coating, dipping and spray coating.
  • the powder RX is distributed on the surface of the magnet evenly.
  • an irregular magnet it is easier to adopt dipping and spray coating to realize the even distribution of the RXE layer.
  • the grain size of the heave rare earth powder RX is less than 30 ⁇ m and the thickness of the RXE layer ranges from 10 ⁇ m to 200 ⁇ m.
  • the grain size of RX particles is greater than 30 ⁇ m, it is easy for RX to settle and not easy to form the slurry RXE with high uniformity. Therefore, it is harder to form an RXE layer on the surface of the magnet.
  • the coating is thinner it is easy to form granular bulges on the coating surface and then the diffusion uniformity of the magnet will finally be affected.
  • the thickness of the RXE layer is controlled within a certain range because when the RXE layer is too thin the grain size of the RX particles in the RXE layer is close to the thickness of the coating and it is harder to realize even distribution of the RX particles. Therefore, the heavy rare earth elements which diffuse into the interior of the magnet from the surface of the magnet are not even in distribution, and finally the uniformity of the magnet is poor.
  • the RXE layer is too thick, the RXE layer has excessive RX.
  • the excessive RX cannot entirely diffuse into the interior of the magnet during heat treatment, gathers on the surface of the magnet, corrodes the surface of the magnet, and affects the surface condition of the magnet.
  • the RXE layer is too thick, the RXE layer has excessive EP and ET. Therefore, a lot of organic materials come out during heat treatment. If the excessive EP and ET cannot be discharged in time, the air of heat treatment equipment will be affected, the content of carbon and oxygen in the magnet will increase and the magnet performance will be finally affected.
  • the organic solvent ET is one or more of ethanol, benzene, glycerol and ethanediol and the ethanol is the preferred one. Compared to ethanol, benzene, glycerol and ethanediol are more harmful to human bodies. During solidification and heat treatment, a lot of ET will fall off at a high temperature. If benzene, glycerol and ethanediol are used as an organic solvent ET, they have higher requirements on the air tightness, air-discharging capacity and safety of equipment. Therefore, the cost of equipment increases.
  • the treated magnet at least has one direction with thickness less than 10 mm.
  • the heavy rare earth element RX diffuses into the interior of the magnet through liquid-like grain boundaries.
  • the diffusion is mainly driven by concentration differences. If the concentration difference is lower, the driving force is not strong and then the diffusion is slow.
  • the magnet thickness is greater than 10 mm, it is very hard to realize full diffusion, and then the magnetic properties like Hk/Hcj become poor, and finally the temperature resistance of the magnet is affected.
  • the invention uses the heavy rare earth element powder RX, organic solid EP and organic solvent ET to prepare slurry RXE which is arranged on the surface of the magnet. After drying treatment, an RXE layer is formed on the surface of the magnet to realize the arrangement of heavy rare earth elements on the surface of the magnet, and then the magnet can be stored stably in the air for a long time. During heat treatment, the organic solid powder EP and the organic solvent ET are separated from the magnet so the content of carbon in the magnet will not increase obviously.
  • the heavy rare earth elements in the heavy rare earth element powder RX diffuse into the interior of the magnet and realize grain boundary diffusion to improve magnet properties.
  • the slurry RXE can be arranged on the surface of the magnet through brush coating, dipping, roller coating and spray coating. The thickness of the RXE layer is controllable. It is easy to realize automatic production.
  • Raw materials were melted in a vacuum melting furnace under the protection of inert gas to form R—Fe—B alloy scales with the thickness ranging from 0.1 mm to 0.5 mm.
  • the metallographic grain boundaries of the scales were clear.
  • the alloy scales were ground by nitrogen gas flow until the surface mean diameter (SMD) was 3.2 ⁇ m.
  • SMD surface mean diameter
  • the 15 KOe magnetic field orientation was adopted for compression molding to produce pressings.
  • the density of the pressings was 3.95 g/cm 3 .
  • the pressings were sintered in a vacuum in a sintering furnace. The pressings were sintered at the highest temperature of 1080° C. for 330 minutes to produce green pressings.
  • the green pressings become magnetic sheets.
  • the size of the magnetic sheets was 40 mm*30 mm*2.1 mm and the size tolerance was ⁇ 0.03 mm.
  • the surface of the magnetic sheets was washed by acid solutions and deionized water. After drying treatment, a treated magnet M1 was produced.
  • the composition of the treated magnet M1 is shown in Table 2 below.
  • Heavy rare earth element powder TbH, organic solid rosin-modified alkyd resin powder and ethanol were mixed to prepare a slurry RXE.
  • the weight percents of the TbH, the rosin-modified alkyd resin powder and the ethanol were 60 wt. %, 5 wt. % and 35 wt. %, respectively.
  • Stir the slurry RXE for about 60 minutes. Dip the treated magnet M1 in the slurry RXE for about 3 seconds and then take the treated magnet M1 out. Put the treated magnet M1 in a drying oven at a temperature of 70° C. for about 15 minutes to produce the treated magnet with an RXE layer on the surface.
  • the treated magnet with an RXE layer in a material box for heat treatment in heat treatment equipment. After the temperature rose to 920° C., keep the magnet at the temperature of 920° C. for 18 hours and then chill the magnet quickly. Then, the temperature rose to 500° C. for aging treatment (the aging treatment refers to the heat treatment process that the properties, shapes and sizes of alloy work pieces after solution treatment, cold plastic deformation or casting and forging change with time at a higher temperature or the room temperature). Keep the magnet at a temperature of 500° C. for 4 hours and then chill the magnet quickly to the room temperature to produce the magnet M2.
  • the aging treatment refers to the heat treatment process that the properties, shapes and sizes of alloy work pieces after solution treatment, cold plastic deformation or casting and forging change with time at a higher temperature or the room temperature.
  • the residual magnetism Br of the magnet M2 is reduced by about 190 Gs, and the Hcj of the magnet M2 increases by about 9.33 KOe through this method.
  • Tb of the magnet M2 increases by about 0.48 wt. %.
  • Table 3 shows the comparison of the CSON element content of the magnet before and after diffusion treatment.
  • Raw materials were melted in a vacuum melting furnace under the protection of inert gas to form R—Fe—B alloy scales with the thickness ranging from 0.1 mm to 0.5 mm.
  • the metallographic grain boundaries of the scales were clear.
  • the alloy scales were ground by nitrogen gas flow until the surface mean diameter (SMD) was 3.1 ⁇ m.
  • SMD surface mean diameter
  • the 15 KOe magnetic field orientation was adopted for compression molding to produce pressings.
  • the density of the pressings was 3.95 g/cm 3 .
  • the pressings were sintered in a vacuum in a sintering furnace. The pressings were sintered at the highest temperature of 1085° C. for 330 minutes to produce green pressings.
  • the green pressings become magnetic sheets.
  • the size of the magnetic sheets was 40 mm*30 mm*3 mm and the size tolerance was ⁇ 0.03 mm.
  • the surface of the magnetic sheets was washed by acid solutions and deionized water. After drying treatment, a treated magnet M3 was produced.
  • the composition of the treated magnet M3 is shown in Table 5 below.
  • Heavy rare earth element powder TbF, polyvinyl butyral and ethanol were mixed to prepare a slurry RXE.
  • the weight percents of the TbF, the polyvinyl butyral and the ethanol were 65 wt. %, 6 wt. % and 29 wt. %, respectively.
  • Stir the slurry RXE for about 60 minutes. Dip the treated magnet M3 in the slurry RXE for about 3 seconds and then take the treated magnet M3 out. Put the treated magnet M3 in a drying oven at a temperature of 70° C. for about 15 minutes to produce the treated magnet with an RXE layer on the surface.
  • the residual magnetism Br of the magnet M4 is reduced by about 170 Gs, and the Hcj of the magnet M4 increases by about 9.86 KOe through this method.
  • Tb of the magnet M4 increases by about 0.48 wt. %.
  • Table 6 shows the comparison of the CSON element content of the magnet before and after diffusion treatment.
  • Raw materials were melted in a vacuum melting furnace under the protection of inert gas to form R—Fe—B alloy scales with the thickness ranging from 0.1 mm to 0.5 mm.
  • the metallographic grain boundaries of the scales were clear.
  • the alloy scales were ground by jet milling to yield powders having the surface mean diameter (SMD) of 3.2 ⁇ m.
  • SMD surface mean diameter
  • the 15 KOe magnetic field orientation was adopted for compression molding to produce pressings.
  • the density of the pressings was 3.95 g/cm 3 .
  • the pressings were sintered in a vacuum in a sintering furnace.
  • the pressings were sintered at the highest temperature of 1085° C. for 300 minutes to produce green pressings. After wire-electrode cutting, the green pressings become magnetic sheets.
  • the size of the magnetic sheets was 40 mm*25 mm*4.5 mm and the size tolerance was ⁇ 0.03 mm.
  • the surface of the magnetic sheets was washed by acid solutions and deionized water. After drying treatment, a treated magnet M5 was produced.
  • the composition of the treated magnet M5 is shown in Table 8 below.
  • Heavy rare earth element powders TbF and Tb, organic solid urea resin and ethanol were mixed to prepare a slurry RXE, and the weight percents thereof were 60 wt. %, 6 wt. % and 34 wt. %, respectively.
  • the maximum particle size of the mixed powders of TbF and Tb was less than 18 ⁇ m.
  • the treated magnet M5 was coated with a layer of RXE slurry. Put the treated magnet M5 in a drying oven at a temperature of 90° C. for about 15 minutes to produce the treated magnet with an RXE layer on the surface.
  • the weight of the treated magnet M5 was increased by 1.02 wt. %.
  • the holding time for thermal treatment at 930° C. is significantly longer than that in examples 1 and 2.
  • Table 9 shows the comparison of the CSON element content of the magnet before and after diffusion treatment.

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  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Environmental & Geological Engineering (AREA)
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  • Manufacturing Cores, Coils, And Magnets (AREA)
  • Metallurgy (AREA)
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US15/690,238 2016-08-31 2017-08-29 Method for producing a sintered r-iron-boron magnet Abandoned US20180061540A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201610776183.5A CN106158347B (zh) 2016-08-31 2016-08-31 一种制备R‑Fe‑B类烧结磁体的方法
CN201610776183.5 2016-08-31

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US (1) US20180061540A1 (fr)
EP (1) EP3291264B1 (fr)
JP (1) JP6595542B2 (fr)
KR (1) KR101906068B1 (fr)
CN (1) CN106158347B (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
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US20210296049A1 (en) * 2020-03-17 2021-09-23 Ningbo Jinji Strong Magnetic Material Co., Ltd. COATING MATERIALS FOR DIFFUSING INTO MAGNET OF NdFeB AND A METHOD OF MAKING IT
CN114823118A (zh) * 2022-06-27 2022-07-29 宁波科宁达工业有限公司 一种稀土永磁体及其制备方法
CN119252635A (zh) * 2024-09-09 2025-01-03 安徽大学 一种晶界扩散钕铁硼磁体基材及晶界扩散钕铁硼磁体的制备方法

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CN107026003B (zh) * 2017-04-24 2020-02-07 烟台正海磁性材料股份有限公司 一种烧结钕铁硼磁体的制备方法
CN107516595A (zh) * 2017-09-19 2017-12-26 江苏晨朗电子集团有限公司 一种用于烧结钕铁硼产品的表面渗镝、铽工艺及搅拌装置
CN108461272B (zh) * 2018-03-20 2020-05-22 北京工业大学 一种用于形成氢化物纳米颗粒表面涂层的技术
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CN108831655B (zh) * 2018-07-20 2020-02-07 烟台首钢磁性材料股份有限公司 一种提高钕铁硼烧结永磁体矫顽力的方法
CN108962582B (zh) * 2018-07-20 2020-07-07 烟台首钢磁性材料股份有限公司 一种钕铁硼磁体矫顽力提升方法
CN109887696B (zh) * 2019-01-15 2021-01-29 宁波金鸡强磁股份有限公司 一种涂覆于钕铁硼磁体的有机浆料及高矫顽力钕铁硼磁体的制备
CN109935462B (zh) * 2019-03-12 2022-02-11 宁波雄海稀土速凝技术有限公司 晶界扩散重稀土钕铁硼磁体的制备方法及其钕铁硼磁体
JP7331470B2 (ja) * 2019-06-04 2023-08-23 Tdk株式会社 R‐t‐b系永久磁石の製造方法
CN110517882B (zh) * 2019-08-15 2021-06-18 安徽省瀚海新材料股份有限公司 一种钕铁硼表面渗铽方法
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CN111243807B (zh) * 2020-02-26 2021-08-27 厦门钨业股份有限公司 一种钕铁硼磁体材料、原料组合物及制备方法和应用
CN113035483B (zh) * 2021-04-23 2024-06-04 宁波佳丰磁材科技有限公司 一种晶界扩散钕铁硼磁铁及其制备方法
CN115602399B (zh) 2021-06-28 2025-11-14 烟台正海磁性材料股份有限公司 一种R-Fe-B烧结磁体及其制备方法和应用
CN113593800B (zh) * 2021-07-20 2023-01-10 烟台正海磁性材料股份有限公司 一种高性能烧结钕铁硼磁体及其制备方法
CN120126887A (zh) * 2025-03-20 2025-06-10 宁波科宁达工业有限公司 一种钕铁硼系磁体、磁体基体及钕铁硼系磁体的制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010238712A (ja) * 2009-03-30 2010-10-21 Tdk Corp 希土類焼結磁石の製造方法
US20120139388A1 (en) * 2010-03-04 2012-06-07 Tdk Corporation Rare earth sintered magnet and motor
EP2555207A1 (fr) * 2010-03-30 2013-02-06 TDK Corporation Aimant fritté de terre rare, procédé de production associé, moteur et automobile
CN103646773A (zh) * 2013-11-21 2014-03-19 烟台正海磁性材料股份有限公司 一种R-Fe-B类烧结磁体的制造方法
WO2015156074A1 (fr) * 2014-04-08 2015-10-15 トヨタ自動車株式会社 Composition de pâte épaisse non magnétique et procédé de production d'un aimant en terres rares

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005344165A (ja) * 2004-06-03 2005-12-15 Tdk Corp 希土類焼結磁石の製造方法、熱処理方法
EP1830371B1 (fr) * 2004-10-19 2016-07-27 Shin-Etsu Chemical Co., Ltd. Procede de preparation d'un materiau pour aimant permanent en terre rare
TWI413136B (zh) 2005-03-23 2013-10-21 Shinetsu Chemical Co 稀土族永久磁體
CN103295713B (zh) 2006-01-31 2016-08-10 日立金属株式会社 R-Fe-B类稀土烧结磁铁
CN101651038B (zh) 2006-03-03 2012-06-06 日立金属株式会社 扩散处理装置
JP4840606B2 (ja) 2006-11-17 2011-12-21 信越化学工業株式会社 希土類永久磁石の製造方法
EP2892063B1 (fr) * 2012-08-31 2018-08-15 Shin-Etsu Chemical Co., Ltd. Procédé de production d'aimant permanent aux terres rares
US10179955B2 (en) * 2012-08-31 2019-01-15 Shin-Etsu Chemical Co., Ltd. Production method for rare earth permanent magnet
CN103258633B (zh) * 2013-05-30 2015-10-28 烟台正海磁性材料股份有限公司 一种R-Fe-B系烧结磁体的制备方法
US10109403B2 (en) * 2013-08-09 2018-10-23 Tdk Corporation R-T-B based sintered magnet and motor
WO2015058654A1 (fr) * 2013-10-22 2015-04-30 北京中科三环高技术股份有限公司 Composition de poudre et procédé de préparation d'un aimant fritté de la série r-fe-b
CN105070498B (zh) * 2015-08-28 2016-12-07 包头天和磁材技术有限责任公司 提高磁体矫顽力的方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010238712A (ja) * 2009-03-30 2010-10-21 Tdk Corp 希土類焼結磁石の製造方法
US20120139388A1 (en) * 2010-03-04 2012-06-07 Tdk Corporation Rare earth sintered magnet and motor
EP2555207A1 (fr) * 2010-03-30 2013-02-06 TDK Corporation Aimant fritté de terre rare, procédé de production associé, moteur et automobile
CN103646773A (zh) * 2013-11-21 2014-03-19 烟台正海磁性材料股份有限公司 一种R-Fe-B类烧结磁体的制造方法
WO2015156074A1 (fr) * 2014-04-08 2015-10-15 トヨタ自動車株式会社 Composition de pâte épaisse non magnétique et procédé de production d'un aimant en terres rares

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210296049A1 (en) * 2020-03-17 2021-09-23 Ningbo Jinji Strong Magnetic Material Co., Ltd. COATING MATERIALS FOR DIFFUSING INTO MAGNET OF NdFeB AND A METHOD OF MAKING IT
US11848152B2 (en) * 2020-03-17 2023-12-19 Ningbo Jinji Strong Magnetic Material Co., Ltd. Coating materials for diffusing into magnet of NdFeB and a method of making it
CN114823118A (zh) * 2022-06-27 2022-07-29 宁波科宁达工业有限公司 一种稀土永磁体及其制备方法
CN119252635A (zh) * 2024-09-09 2025-01-03 安徽大学 一种晶界扩散钕铁硼磁体基材及晶界扩散钕铁硼磁体的制备方法

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